反应详情

14.0 G. of 2,4-dimethyl-3-hydroxymethyl-5-(methylthio)thiophene and 26.0 G. of triphenylphosphonium bromide were dissolved in 75 ml. of acetonitrile and stirred at 40° C. for 1 hour. The resulting mixture was cooled and poured into 150 ml. of ethyl acetate then treated with ethyl ether/hexane (5:1). The resulting solution was decanted from a gum-like residue. The residue was treated with hot acetone and the resulting white crystals were filtered, washed with cold acetone and dried under high vacuum at 80° C. to yield [2,4-dimethyl-5-(methylthio)-3-thenyl]triphenylphosphonium bromide, m.p. 245°-248° C.

1. temperatureThe resulting mixture was cooled
2. additionpoured into 150 ml
3. customThe resulting solution was decanted from a gum-like residue
4. additionThe residue was treated with hot acetone
5. filtrationthe resulting white crystals were filtered
6. washwashed with cold acetone
7. customdried under high vacuum at 80° C.